CN114225453A - Device and method for extracting furfuryl alcohol by rectification in maltol production - Google Patents
Device and method for extracting furfuryl alcohol by rectification in maltol production Download PDFInfo
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- CN114225453A CN114225453A CN202111419936.4A CN202111419936A CN114225453A CN 114225453 A CN114225453 A CN 114225453A CN 202111419936 A CN202111419936 A CN 202111419936A CN 114225453 A CN114225453 A CN 114225453A
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- rectifying tower
- rectifying
- furfuryl alcohol
- tower
- plate heat
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- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 title claims abstract description 141
- XPCTZQVDEJYUGT-UHFFFAOYSA-N 3-hydroxy-2-methyl-4-pyrone Chemical compound CC=1OC=CC(=O)C=1O XPCTZQVDEJYUGT-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 26
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- HYMLWHLQFGRFIY-UHFFFAOYSA-N Maltol Natural products CC1OC=CC(=O)C1=O HYMLWHLQFGRFIY-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229940043353 maltol Drugs 0.000 title claims abstract description 14
- 238000004821 distillation Methods 0.000 claims abstract description 27
- 238000005086 pumping Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 230000007062 hydrolysis Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 62
- 238000007689 inspection Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000003747 Grignard reaction Methods 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4205—Reflux ratio control splitter
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0003—Condensation of vapours; Recovering volatile solvents by condensation by using heat-exchange surfaces for indirect contact between gases or vapours and the cooling medium
- B01D5/0015—Plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0036—Multiple-effect condensation; Fractional condensation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/38—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with substituted hydrocarbon radicals attached to ring carbon atoms
- C07D307/40—Radicals substituted by oxygen atoms
- C07D307/42—Singly bound oxygen atoms
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Apparatus Associated With Microorganisms And Enzymes (AREA)
Abstract
A device and a method for extracting furfuryl alcohol by rectification in maltol production are disclosed: pumping the intermediate of the Grignard hydrolysis kettle into three rectifying towers connected in series, heating the intermediate by two plate heat exchangers in the period, pumping one part of the outlet pump of the first rectifying tower into the second rectifying tower, returning the other part of the outlet pump of the first rectifying tower to the inlet of the second plate heat exchanger, and feeding the solvent distilled from the tops of the first rectifying tower and the second rectifying tower into a rectifying receiving tank; and (3) collecting furfuryl alcohol from the bottom of the third distillation tower, feeding the furfuryl alcohol into the first plate heat exchanger as a heat source to heat the intermediate raw material of the Grignard hydrolysis kettle, simultaneously cooling the furfuryl alcohol, feeding the furfuryl alcohol into a furfuryl alcohol transfer storage tank, feeding the furfuryl alcohol into the next working section after the furfuryl alcohol is qualified, and feeding a solvent distilled from the top of the third distillation tower into the first distillation tower to control the temperature and the liquid level of the first distillation tower. Compared with the prior art, the method has the advantages that the rectification process is only needed, the process is greatly reduced, the production efficiency is improved, and the method is more environment-friendly.
Description
Technical Field
The invention relates to a device and a method for extracting furfuryl alcohol by rectification in maltol production.
Background
The production process of maltol is divided into a Grignard working section, a chlorination working section, a sublimation working section, a crystallization working section and a drying working section; wherein the Grignard section comprises Grignard reaction, addition reaction, hydrolysis reaction, rectification and reduced distillation. The last two procedures are that recovering solvent to extract furfuryl alcohol, rectifying and concentrating, then pumping to a reduced pressure distillation kettle to perform reduced pressure distillation to recover the solvent, heating the reduced pressure distillation kettle to 85-90 ℃, finally cooling by circulating water, placing into a furfuryl alcohol transfer storage tank after sampling and analyzing are qualified, relating to two procedures, and the procedures are complex and are not beneficial to continuous operation.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a device for rectifying and extracting furfuryl alcohol in maltol production, which has a simple structure and obviously shortens the technical process compared with the prior art.
The second technical problem to be solved by the invention is to provide the method for rectifying furfuryl alcohol by the device for rectifying and extracting furfuryl alcohol in maltol production, which has the advantages of simple steps, low energy consumption and capability of effectively improving the efficiency.
In order to solve the first technical problem, the invention provides a device for extracting furfuryl alcohol by rectification in maltol production, which comprises an intermediate tank, three rectification towers, two plate heat exchangers, a rectification receiving tank and a furfuryl alcohol transfer storage tank;
the middle part of each rectifying tower is provided with a material inlet, the upper part of each rectifying tower is provided with a distillation outlet, and the lower part of each rectifying tower is provided with a material outlet;
each plate heat exchanger is provided with a material inlet, a material outlet, and an inlet and an outlet of a heat exchange medium;
a discharge port of the intermediate tank is connected with a material inlet of the first plate heat exchanger through a first pump, a material outlet of the first plate heat exchanger is connected with a material inlet of the second plate heat exchanger, a material outlet of the second plate heat exchanger is connected with a material inlet of the first rectifying tower, a material outlet of the first rectifying tower is connected with a material inlet of the second rectifying tower through a second pump, an outlet end of the second pump is provided with a branch pipe, the other end of the branch pipe is connected with a material inlet of the second plate heat exchanger, a material outlet of the second rectifying tower is connected with a material inlet of the third rectifying tower through a third pump, a material outlet of the third rectifying tower is connected with a heat exchange medium inlet of the first plate heat exchanger, a heat exchange outlet of the first plate heat exchanger is connected with a furfuryl alcohol transfer storage tank, a distillation outlet of the third rectifying tower is connected with a material inlet of the first rectifying tower, the distillation outlet of the second rectifying tower is connected with the rectifying receiving tank.
Preferably, the second plate heat exchanger, the second rectifying tower and the third rectifying tower are respectively connected with a reboiler to be heated by steam, and the first rectifying tower is heated by steam condensate generated by the second rectifying tower, the third rectifying tower and other sections.
In order to solve the second technical problem, the present invention provides a method for rectifying furfuryl alcohol by using an apparatus for rectifying furfuryl alcohol in maltol production, comprising the following steps:
(1) the intermediate of the Grignard hydrolysis kettle is put into an intermediate tank and then pumped into a first rectifying tower by a first pump, and is heated by a first plate heat exchanger and a second plate heat exchanger during the process, and the flow rate is controlled to be 4.5-5m3H, pumping one part of the material at the bottom of the first rectifying tower into the second rectifying tower through a second pump, returning the other part of the material to a material inlet of the second plate heat exchanger, and keeping the flow velocity of the material entering the second rectifying tower to be 3-3.5m by adjusting the flow of each part3H, the tower bottom temperature of the first rectifying tower is not lower than 45 ℃;
(2) controlling the bottom temperature of the second rectifying tower to be 65-70 ℃, pumping the materials at the bottom of the second rectifying tower into a third rectifying tower through a third pump at the flow rate of 1.0-1.5m3/h, and feeding the solvents distilled from the tops of the first rectifying tower and the second rectifying tower into a rectifying receiving tank;
(3) controlling the temperature of the bottom of the third distillation tower to be 85-90 ℃, extracting furfuryl alcohol from the bottom of the third distillation tower at the flow rate of 600-plus 800L/h, taking the furfuryl alcohol as a heat source, entering a first plate heat exchanger to heat the intermediate raw material of the Grignard hydrolysis kettle, simultaneously cooling the furfuryl alcohol, entering a furfuryl alcohol transfer storage tank, entering the next working section after the furfuryl alcohol is qualified through inspection, and entering a solvent distilled from the top of the third distillation tower into the first distillation tower to control the temperature and the liquid level of the first distillation tower.
The invention has the advantages that: compared with the prior art that furfuryl alcohol is obtained by the intermediate through two procedures of rectification and reduced evaporation, the method only needs a rectification procedure at present, obviously reduces the procedures, improves the production efficiency, and is more energy-saving and environment-friendly by using the generated furfuryl alcohol as a heat source of the first plate heat exchanger and heating the first rectification tower through the second rectification tower, the third rectification tower and steam condensate generated in other working sections.
Drawings
FIG. 1 is a schematic flow diagram of the present invention.
Detailed Description
Referring to fig. 1, a device for extracting furfuryl alcohol by rectification in maltol production comprises an intermediate tank 1, three rectification towers 2a/2b/2c, two plate heat exchangers 3a/3b, a rectification receiving tank 4 and a furfuryl alcohol transfer storage tank 5;
the middle part of each rectifying tower 2a/2b/2c is provided with a material inlet, the upper part is provided with a distillation outlet, and the lower part is provided with a material outlet;
each plate heat exchanger 3a/3b is provided with a material inlet, a material outlet, and an inlet and an outlet of a heat exchange medium;
a discharge port of the intermediate tank 1 is connected with a material inlet of a first plate heat exchanger 3a through a first pump 6, a material outlet of the first plate heat exchanger 3a is connected with a material inlet of a second plate heat exchanger 3b, a material outlet of the second plate heat exchanger 3b is connected with a material inlet of a first rectifying tower 2a, a material outlet of the first rectifying tower 2a is connected with a material inlet of the second rectifying tower 2b through a second pump 7, a branch pipe 9 (the branch pipe 9 is used for controlling flow) is arranged at an outlet end of the second pump 7, the other end of the branch pipe 9 is connected with a material inlet of the second plate heat exchanger 3b, a material outlet of the second rectifying tower 2b is connected with a material inlet of a third rectifying tower 2c through a third pump 8, a material outlet of the third rectifying tower 2c is connected with a heat exchange medium inlet of the first plate heat exchanger 3a, a heat exchange outlet of the first plate heat exchanger 3a is connected with a furfuryl alcohol transfer storage tank 5, the distillation outlet of the third rectifying tower 2c is connected with the material inlet of the first rectifying tower 2a, and the distillation outlets of the first rectifying tower 2a and the second rectifying tower 2b are connected with the rectification receiving tank 4.
The second plate heat exchanger 3b, the second rectifying tower 2b and the third rectifying tower 2c are respectively connected with a reboiler to be heated by steam, and the first rectifying tower 2a is heated by steam condensate generated by the second rectifying tower 2b, the third rectifying tower 2c and other sections.
A method for rectifying furfuryl alcohol by a device for rectifying and extracting furfuryl alcohol in maltol production comprises the following steps:
(1) the intermediate of the Grignard hydrolysis kettle is put into the intermediate tank 1 and then pumped into the first rectifying tower 2a by a first pump 6, and is heated by the first plate heat exchanger 3a and the second plate heat exchanger 3b in the process, and the flow rate is controlled to be 4.5-5m3H, pumping one part of the material at the bottom of the first rectifying tower 2a into the second rectifying tower 2b through a second pump 7, returning the other part of the material to a material inlet of the second plate heat exchanger 3b, and keeping the flow velocity entering the second rectifying tower 2b to be 3-3.5m by adjusting the flow of each part3H, and the temperature of the bottom of the first rectifying tower 2a is not lower than 45 ℃;
(2) controlling the temperature of the bottom of the second rectifying tower 2b to be 65-70 ℃, and feeding the material at the bottom of the second rectifying tower 2b by a third pump 8 in a range of 1.0-1.5m3Pumping the solvent distilled from the tops of the first rectifying tower 2a and the second rectifying tower 2b into a rectifying receiving tank 4 at a flow rate of/h;
(3) controlling the temperature of the bottom of the third rectifying tower 2c to be 85-90 ℃, extracting furfuryl alcohol from the bottom of the third rectifying tower 2c at the flow rate of 600-.
The invention has the advantages that: compared with the prior art that furfuryl alcohol is obtained by the intermediate through two procedures of rectification and reduced evaporation, the rectification procedure is only needed at present, the procedures are obviously reduced, the production efficiency is improved, in addition, the generated furfuryl alcohol is used as a heat source of the first plate heat exchanger 3a, and the first rectification tower 2a is heated through the second rectification tower 2b, the third rectification tower 2c and steam condensate generated in other working sections, so that the energy conservation and the environmental protection are realized.
Claims (3)
1. A device for rectifying and extracting furfuryl alcohol in maltol production is characterized in that: comprises an intermediate tank, three rectifying towers, two plate heat exchangers, a rectifying receiving tank and a furfuryl alcohol transfer storage tank;
the middle part of each rectifying tower is provided with a material inlet, the upper part of each rectifying tower is provided with a distillation outlet, and the lower part of each rectifying tower is provided with a material outlet;
each plate heat exchanger is provided with a material inlet, a material outlet, and an inlet and an outlet of a heat exchange medium;
a discharge port of the intermediate tank is connected with a material inlet of the first plate heat exchanger through a first pump, a material outlet of the first plate heat exchanger is connected with a material inlet of the second plate heat exchanger, a material outlet of the second plate heat exchanger is connected with a material inlet of the first rectifying tower, a material outlet of the first rectifying tower is connected with a material inlet of the second rectifying tower through a second pump, an outlet end of the second pump is provided with a branch pipe, the other end of the branch pipe is connected with a material inlet of the second plate heat exchanger, a material outlet of the second rectifying tower is connected with a material inlet of the third rectifying tower through a third pump, a material outlet of the third rectifying tower is connected with a heat exchange medium inlet of the first plate heat exchanger, a heat exchange outlet of the first plate heat exchanger is connected with a furfuryl alcohol transfer storage tank, a distillation outlet of the third rectifying tower is connected with a material inlet of the first rectifying tower, the distillation outlet of the second rectifying tower is connected with the rectifying receiving tank.
2. The apparatus for fractionating furfuryl alcohol in maltol production according to claim 1, wherein: the second plate heat exchanger, the second rectifying tower and the third rectifying tower are respectively connected with a reboiler and heated by steam, and the first rectifying tower is heated by steam condensate generated by the second rectifying tower, the third rectifying tower and other sections.
3. The method for rectifying furfuryl alcohol by the device for rectifying furfuryl alcohol in maltol production as claimed in claim 1 or 2, comprising the steps of:
(1) the intermediate of the Grignard hydrolysis kettle is put into an intermediate tank and then pumped into a first rectifying tower by a first pump, and is heated by a first plate heat exchanger and a second plate heat exchanger during the process, and the flow rate is controlled to be 4.5-5m3H, pumping one part of the material at the bottom of the first rectifying tower into the second rectifying tower through a second pump, returning the other part of the material to a material inlet of the second plate heat exchanger, and keeping the flow velocity of the material entering the second rectifying tower to be 3-3.5m by adjusting the flow of each part3H, the tower bottom temperature of the first rectifying tower is not lower than 45 ℃;
(2) controlling the bottom temperature of the second rectifying tower to be 65-70 ℃, pumping the materials at the bottom of the second rectifying tower into a third rectifying tower through a third pump at the flow rate of 1.0-1.5m3/h, and feeding the solvents distilled from the tops of the first rectifying tower and the second rectifying tower into a rectifying receiving tank;
(3) controlling the temperature of the bottom of the third distillation tower to be 85-90 ℃, extracting furfuryl alcohol from the bottom of the third distillation tower at the flow rate of 600-plus 800L/h, taking the furfuryl alcohol as a heat source, entering a first plate heat exchanger to heat the intermediate raw material of the Grignard hydrolysis kettle, simultaneously cooling the furfuryl alcohol, entering a furfuryl alcohol transfer storage tank, entering the next working section after the furfuryl alcohol is qualified through inspection, and entering a solvent distilled from the top of the third distillation tower into the first distillation tower to control the temperature and the liquid level of the first distillation tower.
Priority Applications (1)
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CN202111419936.4A CN114225453A (en) | 2021-11-26 | 2021-11-26 | Device and method for extracting furfuryl alcohol by rectification in maltol production |
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CN202111419936.4A CN114225453A (en) | 2021-11-26 | 2021-11-26 | Device and method for extracting furfuryl alcohol by rectification in maltol production |
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2021
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